[μ-2-(4-Hy­droxy­phen­yl)acetato]-κ3 O:O,O′;κ3 O,O′:O′-bis­{aqua­(4,4′-bi­pyridine-κN)bis­[2-(4-hy­droxy­phen­yl)acetato-κ2 O,O′]holmium(III)} mono­hydrate

Jia-Lu Liu; Jian-Feng Liu; Guo-Liang Zhao

doi:10.1107/S1600536811001115

. 2011 Jan 15;67(Pt 2):m191–m192. doi: 10.1107/S1600536811001115

[μ-2-(4-Hydroxyphenyl)acetato]-κ³ O:O,O′;κ³ O,O′:O′-bis{aqua(4,4′-bipyridine-κN)bis[2-(4-hydroxyphenyl)acetato-κ² O,O′]holmium(III)} monohydrate

Jia-Lu Liu ^a, Jian-Feng Liu ^a, Guo-Liang Zhao ^a,^*

PMCID: PMC3051499 PMID: 21522861

Abstract

In the title dinuclear complex, [Ho₂(C₈H₇O₃)₆(C₁₀H₈N₂)₂(H₂O)₂]·H₂O, each of the two independent Ho^III ions is coordinated by eight O atoms from four 4-hydroxyphenylacetate (HPAA) ligands and a water molecule, and one N atom from a 4,4′-bipyridine (bipy) ligand in a distorted tricapped trigonal–prismatic geometry. The HPAA ligands are coordinated in bis-chelate, bridging and bridging tridentate modes. In the crystal, O—H⋯O and O—H⋯N hydrogen bonds link the molecules into a three-dimensional network.

Related literature

For background to the importance of coordination modes in magnetic structures, see: Fang & Zhang (2006 ▶); Munoz et al. (2005 ▶); Wang & Sevov (2008 ▶); Wang et al. (2010 ▶). For a related structure, see: Liu et al. (2010 ▶).

Experimental

Crystal data

[Ho₂(C₈H₇O₃)₆(C₁₀H₈N₂)₂(H₂O)₂]·H₂O
M _r = 1603.09
Triclinic,
a = 11.7217 (7) Å
b = 16.1885 (9) Å
c = 18.413 (1) Å
α = 83.441 (3)°
β = 72.208 (3)°
γ = 71.337 (3)°
V = 3151.4 (3) Å³
Z = 2
Mo Kα radiation
μ = 2.58 mm⁻¹
T = 296 K
0.34 × 0.11 × 0.03 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.469, T _max = 0.924
49489 measured reflections
14593 independent reflections
12826 reflections with I > 2σ(I)
R _int = 0.021

Refinement

R[F ² > 2σ(F ²)] = 0.019
wR(F ²) = 0.051
S = 1.00
14593 reflections
874 parameters
9 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.58 e Å⁻³
Δρ_min = −0.66 e Å⁻³

Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: SAINT (Bruker, 2006 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811001115/lx2179sup1.cif

e-67-0m191-sup1.cif^{(64.8KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811001115/lx2179Isup2.hkl

e-67-0m191-Isup2.hkl^{(713.3KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O6—H6B⋯O3Wⁱ	0.82	1.86	2.646 (3)	160
O9—H9A⋯O17ⁱⁱ	0.82	1.86	2.676 (2)	173
O12—H12A⋯O11ⁱⁱⁱ	0.82	1.94	2.748 (2)	168
O15—H15C⋯O6^iv	0.82	1.90	2.714 (2)	174
O18—H18B⋯O9ⁱ	0.82	1.95	2.769 (3)	174
O1W—H1WA⋯O13	0.84 (4)	1.95 (2)	2.736 (2)	156 (3)
O1W—H1WB⋯N4^v	0.83 (2)	1.97 (2)	2.781 (3)	167 (4)
O2W—H2WA⋯O5	0.84 (4)	1.97 (2)	2.735 (2)	150 (3)
O3W—H3WA⋯O1^vi	0.84 (2)	1.95 (2)	2.780 (2)	176 (4)
O2W—H2WB⋯N2ⁱ	0.83 (2)	2.02 (2)	2.835 (3)	166 (4)
O3—H3B⋯O12^v	0.82	2.05	2.735 (3)	141
O3W—H3WB⋯O3	0.83 (4)	2.00 (4)	2.803 (3)	164 (4)

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Symmetry codes: (i) Inline graphic ; (ii) ; (iii) ; (iv) ; (v) ; (vi) .

supplementary crystallographic information

Comment

The design and synthesis of carboxylic mental–organic complexes have been an increasing interest for decades owing to their potential practical applications, such as fluorescence, magnetism (Wang, et al., 2010; Fang, et al., 2006; Wang, et al., 2008). We have worked at it before (Liu, et al., 2010). Herein we report the crystal structure of a new holmium (III) complex with the ligand 4–hydroxyphenylacetate and 4,4'–bipyridine.

In the title dinuclear complex (I), the unique HoIII ion is coordinated by four HPAA ligands, a bipy ligand and a water molecule via eight O atoms and one N atom (see, Fig. 1). The HoIII ion is in a distorted tricapped trigonal prismatic environment. The HPAA ligands coordinate in the bis–chelate, bridging and bridging tridentate modes.

Experimental

All reagents and solvents used were of commercially available quality and without purified before using. p-hydroxyphenylacetic acid(HPAA) (0.456 g, 3 mmol)and sodium hydroxide (0.12 g, 3 mmol) were mixed together in water(10 ml), then Ho[(NO₃)₃](0.351 g, 1 mmol) dissolved in water(10 ml) was added into the above solution, after stirred for an hour, an ethanol(5 ml) solution of 4,4'-bipyridine(0.156 g, 1 mmol) is slowly dripped into the above solution with stirring for three hours. After filtration, the filtrate was allowed to stand at room temperature, and single crystals suitable for X–ray work were obtained after a week.